CN113151885A - Titanium anode for electroplating and preparation method thereof - Google Patents
Titanium anode for electroplating and preparation method thereof Download PDFInfo
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- CN113151885A CN113151885A CN202110275357.0A CN202110275357A CN113151885A CN 113151885 A CN113151885 A CN 113151885A CN 202110275357 A CN202110275357 A CN 202110275357A CN 113151885 A CN113151885 A CN 113151885A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1225—Deposition of multilayers of inorganic material
Abstract
The invention belongs to the technical field of electroplating, and discloses a titanium anode for electroplating and a preparation method thereof. The titanium anode for electroplating comprises a titanium substrate, and an intermediate layer and a surface layer which are sequentially formed on the titanium substrate, wherein the intermediate layer contains oxides of Ru, Ir and Ti; the surface layer contains at least one of oxides of Ta, Nb, Sn, Zr, Ti or Sb; the thickness ratio of the intermediate layer to the surface layer is (5-15): 1. the titanium anode for electroplating provided by the invention can resist the corrosion of chlorine evolution and oxygen evolution environments, can effectively improve the chlorine evolution and oxygen evolution potentials of the titanium anode, reduce the precipitation of oxygen and chlorine in the electroplating process, avoid the too fast consumption of electroplating additives, is beneficial to maintaining the stability of the plating solution and reduce the electroplating cost.
Description
Technical Field
The invention belongs to the technical field of electroplating, and particularly relates to a titanium anode for electroplating and a preparation method thereof.
Background
In the electroplating industry, nickel plating, zinc plating, copper plating and the like are common electroplating processes. In electroplating, the anode is mostly a soluble anode, which plays a role in supplementing the concentration of the main salt. However, in the actual production process, because the anode is subjected to electrochemical dissolution and chemical dissolution simultaneously, and the cathode is accompanied with hydrogen evolution except for metal deposition, the anode efficiency is higher than the cathode efficiency, so that the concentration of main salt and the pH value in the plating solution are increased continuously. In order to control the stability of the plating solution, water needs to be continuously supplemented into the plating solution for dilution; easily cause overflow cylinder; additives also need to be supplemented and maintained in a certain concentration range; at the same time, acid is also needed to maintain the pH value of the plating solution. Therefore, not only is the plating solution required to be frequently monitored, but also the stable operation of electroplating production is not facilitated; but also wastes raw materials and increases the amount of wastewater discharged.
To solve such problems, the amount of soluble anodes is generally reduced by adding insoluble anodes as auxiliary anodes. However, the conventional insoluble anode has a plurality of problems, such as IrTa coating titanium anode, the coating cost is high, the service life is long under the condition of oxygen evolution, but the service life is reduced under the condition of Cl < - >; RuTi-coated titanium anodes, suitable for use under Cl-conditions, but have a relatively short life in an oxygen evolution environment. And the two types of coating titanium anodes have lower oxygen evolution or chlorine evolution potential, oxygen or chlorine is easy to be evolved in the electroplating process, and the two types of coating titanium anodes can accelerate the consumption of electroplating additives and increase the electroplating cost. Generally speaking, the traditional insoluble titanium anode cannot resist the corrosion of chlorine evolution and oxygen evolution environments at the same time; and the overpotential of chlorine evolution and oxygen evolution cannot be simultaneously improved, and the precipitation of oxygen and chlorine is reduced.
Therefore, it is desired to provide a titanium anode for electroplating, which can increase the chlorine evolution and oxygen evolution potentials at the same time and has a long life.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a titanium anode for electroplating, which can simultaneously improve chlorine evolution and oxygen evolution potentials and has long service life.
A titanium anode for electroplating comprises a titanium substrate, and an intermediate layer and a surface layer which are sequentially formed on the titanium substrate,
the intermediate layer comprises oxides of Ru, Ir, and Ti;
the surface layer comprises at least one of an oxide of Ta, Nb, Sn, Zr, Ti or Sb;
the thickness ratio of the intermediate layer to the surface layer is (5-15): 1.
in the titanium anode for electroplating, the intermediate layer is a conductive main body and plays a decisive role in the conductivity and the service life of the titanium anode. The surface layer adopts transition metal oxide, plays an auxiliary role, can simultaneously improve the chlorine evolution and oxygen evolution potentials of the titanium anode, reduces the precipitation amount of chlorine and oxygen in the electroplating process of the titanium anode, and avoids the over-fast consumption of electroplating additives. Meanwhile, the thickness ratio of the intermediate layer to the surface layer needs to be controlled, when the surface layer is too thick, the service life of the titanium anode is shortened, and when the surface layer is too thin, the effects of simultaneously improving the chlorine evolution potential and the oxygen evolution potential of the titanium anode cannot be achieved.
The intermediate layer of the titanium anode for electroplating comprises oxides of Ru, Ir and Ti, wherein the oxide of Ru is favorable for chlorine evolution environment, the oxide of Ir is favorable for oxygen evolution environment, the oxides of Ru and Ir are used as conductive oxides, and the oxide of Ti is inert oxide. Due to Ru4+、Ir4+、Ti4+The three ions have approximate radiuses and belong to rutile oxides, and oxide solid solutions of Ru, Ir and Ti with stable structures can be formed after sintering, and the addition of a proper amount of Ti oxide is beneficial to improving the stability of the titanium anode.
Preferably, the intermediate layer comprises RuO2、IrO2And TiO2(ii) a The surface layer comprises Ta2O5、Nb2O5、SnO2、ZrO2、TiO2Or Sb2O3At least one of (1).
Preferably, the thickness ratio of the intermediate layer to the surface layer is (5-12): 1.
preferably, in the intermediate layer, in terms of molar ratio, Ru: ir: ti is, Ru: ir: ti is (15-40): (2-10): (55-85); further preferred; more preferably, Ru: ir: ti is (20-35): (3-8): (60-75). When the ratio of the metal components is too high or too low, the corrosion resistance of the intermediate layer is remarkably deteriorated, and the life of the titanium anode is remarkably reduced.
Preferably, the thickness of the intermediate layer is 2 to 15 micrometers; further preferably, the thickness of the intermediate layer is 2 to 10 micrometers; more preferably, the thickness of the intermediate layer is 2 to 8 micrometers.
Preferably, the thickness of the surface layer is 0.1 to 1.0 micron; further preferably, the thickness of the surface layer is 0.2 to 0.8 μm.
Preferably, the titanium substrate is TA1 or TA 2.
The invention also provides a preparation method of the titanium anode for electroplating.
Specifically, the preparation method of the titanium anode for electroplating comprises the following steps:
(1) dissolving acids or salts of Ru, Ir and Ti to prepare an intermediate layer coating solution; coating the intermediate layer coating liquid on a titanium substrate, drying and sintering to obtain an intermediate layer;
(2) dissolving at least one of Ta, Nb, Sn, Zr, Ti or Sb salt to prepare surface layer coating liquid; and (2) coating the surface layer coating liquid on the intermediate layer prepared in the step (1), drying and sintering to prepare a surface layer, thus obtaining the titanium anode for electroplating.
Preferably, the coating process in the step (1) and the step (2) is multiple coatings, and drying and sintering are carried out after each coating until the target thickness is reached.
Preferably, the dissolving process in the step (1) and the step (2) is dissolving by using alcohol; further preferably, the alcohol is butanol and/or propanol.
Preferably, the drying temperature in the step (1) and the step (2) is 100-150 ℃; further preferably, the temperature of the drying in the step (1) and the step (2) is 110-.
Preferably, the sintering temperature in the step (1) and the step (2) is 400-600 ℃; preferably, the sintering temperature in the step (1) and the step (2) is 450-500 ℃.
The invention also provides application of the titanium anode for electroplating.
The titanium anode for electroplating is applied to electroplating, such as an auxiliary anode.
Compared with the prior art, the invention has the following beneficial effects:
the titanium anode provided by the invention comprises a titanium substrate, and an intermediate layer and a surface layer which are sequentially formed on the titanium substrate, wherein the intermediate layer is a conductive main body and plays a decisive role in the conductivity and the service life of the titanium anode; the transition metal oxide surface layer plays an auxiliary role, and can simultaneously improve the chlorine evolution and oxygen evolution potentials of the titanium anode; by controlling the thickness ratio of the middle layer to the surface layer and the components of the metal oxides in each layer, the prepared titanium anode can resist the corrosion of chlorine evolution and oxygen evolution environments at the same time, can effectively improve the chlorine evolution and oxygen evolution potentials of the titanium anode, reduce the precipitation of oxygen and chlorine in the electroplating process, avoid the too fast consumption of electroplating additives, be beneficial to maintaining the stability of the electroplating solution and reduce the electroplating cost.
Drawings
FIG. 1 is a graph showing chlorine evolution polarization curves of titanium anodes for plating prepared in example 1 and comparative example 1;
FIG. 2 is a graph showing oxygen evolution polarization curves of titanium anodes for plating prepared in example 1 and comparative example 1;
FIG. 3 is a graph of cell voltage versus time for the enhanced life test of the titanium anodes for plating prepared in example 2 and comparative example 2.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
And (3) degreasing and etching the titanium plate subjected to sand blasting by oxalic acid to obtain a uniform rough surface with the roughness Ra of 4.0-10.0 microns, and cleaning and drying for later use. Preparing an intermediate layer containing a noble metal oxide coating by adopting a thermal decomposition method: firstly, according to the metal molar ratio Ru: ir: and Ti is 25: 5: 70, dissolving ruthenium trichloride, chloroiridic acid and butyl titanate into n-butanol: preparing a coating solution with the total metal concentration of 0.5mol/L from the solution of isopropanol 1:1, brushing the coating solution on a clean titanium plate, drying the titanium plate for 10min at the temperature of 120 ℃, then sintering the titanium plate for 10min at the temperature of 450 ℃, taking out the titanium plate, cooling the titanium plate, and repeating the brushing, drying and sintering steps for 15 times to obtain the intermediate layer with the thickness of about 4.5 microns. Then, coating a surface layer by using a coating solution of the surface layer as follows: dissolving tantalum pentachloride in n-butanol: preparing a coating solution with the metal concentration of 0.2mol/L in a solution with the isopropanol ratio of 1: 1; and (3) coating the surface layer coating solution on the middle layer, drying at 120 ℃ for 10min, sintering at 500 ℃ for 10min, coating 2 layers of the surface layer coating solution with the thickness of about 0.5 micron, and sintering the last layer for 60min to obtain the titanium anode for electroplating.
Example 2
And (3) degreasing and etching the titanium plate subjected to sand blasting by oxalic acid to obtain a uniform rough surface with the roughness Ra of 4.0-10.0 microns, and cleaning and drying for later use. Preparing an intermediate layer containing a noble metal oxide coating by adopting a thermal decomposition method: firstly, according to the metal molar ratio Ru: ir: ti 28: 7: 65, dissolving ruthenium trichloride, chloroiridic acid and butyl titanate into n-butanol: preparing a coating solution with the total metal concentration of 0.6mol/L from a solution with the isopropanol ratio of 1:1, brushing the coating solution on a clean titanium plate, drying the coating solution at the temperature of 120 ℃ for 10min, then sintering the coating solution at the temperature of 450 ℃ for 10min, taking out the coating solution, cooling the coating solution, and repeating the brushing-drying-sintering steps for 9 times to obtain an intermediate layer with the thickness of about 3.0 micrometers; then, coating a surface layer by using a coating solution of the surface layer as follows: dissolving neodymium pentachloride in n-butanol: preparing a coating solution with the metal concentration of 0.3mol/L in a solution with the isopropanol ratio of 1: 1; and (3) coating the surface layer coating solution on the intermediate layer, coating 1 layer of the surface layer coating solution on the intermediate layer, drying the surface layer coating solution at 120 ℃ for 10min, and sintering the surface layer coating solution at 500 ℃ for 60min to obtain the titanium anode for electroplating.
Example 3
And (3) degreasing and etching the titanium plate subjected to sand blasting by oxalic acid to obtain a uniform rough surface with the roughness Ra of 4.0-10.0 microns, and cleaning and drying for later use. Preparing an intermediate layer containing a noble metal oxide coating by adopting a thermal decomposition method: firstly, according to the metal molar ratio Ru: ir: and Ti is 30: 5: 65, dissolving ruthenium trichloride, chloroiridic acid and butyl titanate into n-butanol: preparing a coating solution with the total metal concentration of 0.4mol/L from a solution with the isopropanol ratio of 1:1, brushing the coating solution on a clean titanium plate, drying the coating solution at the temperature of 120 ℃ for 10min, then sintering the coating solution at the temperature of 450 ℃ for 10min, taking out the coating solution, cooling the coating solution, and repeating the brushing-drying-sintering steps for 20 times to obtain an intermediate layer with the thickness of about 5.0 micrometers; then, coating a surface layer by using a coating solution of the surface layer as follows: dissolving tin tetrachloride in n-butanol: preparing a coating solution with the metal concentration of 0.4mol/L in a solution with the isopropanol ratio of 1: 1; and (3) coating the surface layer coating liquid on the middle layer, drying for 10min at 120 ℃, sintering for 10min at 500 ℃, coating 3 layers of the surface layer coating liquid with the thickness of about 0.7 micron, and sintering the last layer for 60min to obtain the titanium anode for electroplating.
Comparative example 1
Comparative example 1 differs from example 1 in that Ta was doped into a RuIrTi coating to prepare Ru: ir: ti: ta 25: 5: 60: 10 quaternary oxide coatings, brushing 17 total layers, were about 5.0 microns thick. The remaining materials and preparation were the same as in example 1.
Comparative example 2
Comparative example 2 differs from example 2 in that the intermediate layer of comparative example 2 has a thickness of about 3.0 microns, but the surface layer is brushed with 4 layers to a thickness of about 1.2 microns.
The remaining materials and preparation were the same as in example 2.
Comparative example 3
Comparative example 3 differs from example 3 in that comparative example 3 does not have a surface layer applied and the titanium anode coating thickness is about 5.0 microns. The remaining materials and preparation were the same as in example 3.
Comparative example 4
Comparative example 4 differs from example 1 in that the intermediate layer was changed to RuO2-TiO2Coating, wherein the molar ratio of metal ions Ru: and Ti is 30: 70 with an intermediate layer thickness of about 4.5 microns. The surface layer was the same as in example 1, and the remaining materials and preparation methods were the same as in example 1.
Product effectiveness testing
The performance of the titanium anodes for plating prepared in examples 1 to 3 and comparative examples 1 to 4 was tested using a three-electrode system.
(1) Oxygen evolution polarization curve test
And (3) testing conditions are as follows: the electrolyte is 1mol/L sulfuric acid solution, the scanning range is 0.4V-2.0V, the scanning speed is 20mV/s, and the reference electrodes are all saturated calomel electrodes.
(2) Chlorine evolution polarization curve test
And (3) testing conditions are as follows: the electrolyte is a saturated sodium chloride solution, the scanning range is 0.4V-2.0V, the scanning speed is 20mV/s, and the reference electrodes are saturated calomel electrodes.
(3) Enhanced life test
And (3) testing conditions are as follows: the current density of the anode is 1A/cm2Electrolyte solution: 50g/L NaCl +200g/LNa2SO4And when the cell voltage rises to 11V at the temperature of 40 ℃, judging that the titanium anode fails, wherein the total electrifying time is the strengthened service life.
The results of chlorine evolution, oxygen evolution potential, and enhanced lifetime of the titanium anodes for plating prepared in examples 1 to 3 and comparative examples 1 to 4 are shown in Table 1.
TABLE 1 chlorine evolution, oxygen evolution potential, and enhanced lifetime of titanium anodes for plating prepared in examples 1 to 3 and comparative examples 1 to 4
| Test items | Example 1 | Comparative example 1 | Example 2 | Comparative example 2 | Example 3 | Comparative example 3 | Comparative example 4 |
| Chlorine evolution potential/V | 1.1121 | 1.0604 | 1.1161 | 1.1192 | 1.1178 | 1.0670 | 1.1153 |
| Oxygen evolution potential V | 1.2728 | 1.2215 | 1.2733 | 1.2785 | 1.2766 | 1.2239 | 1.2603 |
| Enhanced lifetime/h | 62 | 45 | 60 | 49 | 68 | 67 | 13 |
The main parameters for evaluating titanium anodes are chlorine evolution potential, oxygen evolution potential and strengthening life. The higher the chlorine evolution potential and the oxygen evolution potential are, the more difficult chlorine and oxygen are to be separated out in the electroplating process, and the slower the consumption speed of the electroplating additive is. The service life of the titanium anode is directly related to the strengthening service life.
As is clear from table 1, the titanium anode prepared in example 1 has significantly higher chlorine evolution and oxygen evolution potentials than those of comparative example 1, and chlorine and oxygen are not easily evolved during the plating process. Fig. 1 is a graph showing chlorine evolution polarization of the titanium anodes prepared in example 1 and comparative example 1, and fig. 2 is a graph showing oxygen evolution polarization of the titanium anodes prepared in example 1 and comparative example 1. Fig. 1 and 2 also show that, under the same current conditions, the chlorine evolution and oxygen evolution potentials of example 1 are significantly higher than those of comparative example 1. Meanwhile, the strengthening life of the titanium anode for electroplating prepared in comparative example 1 is also reduced by 37.8% compared with that of the titanium anode prepared in example 1, and the strengthening life of the titanium anode prepared in example 1 is longer. It can be seen that even though the metals of the intermediate layer and the surface layer are used, the titanium anode obtained can not achieve good performance without separating the intermediate layer and the surface layer.
Compared with comparative example 2, the titanium anode for plating prepared in example 2 has chlorine evolution and oxygen evolution potentials equivalent to those of comparative example 2, but the lifetime is significantly reduced. FIG. 3 is a graph of cell voltage versus time for the enhanced life test of the titanium anodes for plating prepared in example 2 and comparative example 2. from FIG. 3, it can be seen that the curve of the titanium anode in comparative example 2 is located above that of example 2, and it is also confirmed that the life of the titanium anode in comparative example 2 is significantly lower than that of example 2. It is also very important to control the thickness ratio of the intermediate layer and the surface layer.
Compared with the comparative example 3, the titanium anode prepared in the example 3 has higher chlorine evolution and oxygen evolution potentials, is not easy to evolve chlorine and oxygen in the electroplating process, and has slow consumption speed of the electroplating additive. It can be seen that the performance of the titanium anode is significantly reduced without brushing the surface layer, even when the total coating thickness is comparable.
Compared with the example 1, the chlorine evolution potential and the oxygen evolution potential of the titanium anode prepared in the comparative example 4 are equivalent to those of the titanium anode prepared in the example 1, but the service life is greatly reduced, and the strengthening service life of the titanium anode prepared in the example 1 is 4.7 times that of the titanium anode prepared in the comparative example 4. It can be seen that the choice of interlayer metal is key to improving the enhanced lifetime of the titanium anode.
Claims (10)
1. A titanium anode for electroplating is characterized by comprising a titanium substrate, and an intermediate layer and a surface layer which are sequentially formed on the titanium substrate,
the intermediate layer comprises oxides of Ru, Ir, and Ti;
the surface layer comprises at least one of an oxide of Ta, Nb, Sn, Zr, Ti or Sb;
the thickness ratio of the intermediate layer to the surface layer is (5-15): 1.
2. a titanium anode for plating according to claim 1, characterized in that the thickness ratio of said intermediate layer and said surface layer is (5-12): 1.
3. the titanium anode for plating according to claim 1, wherein, in said intermediate layer, in terms of molar ratio, Ru: ir: ti is (15-40): (2-10): (55-85).
4. The titanium anode for plating according to claim 3, wherein, in said intermediate layer, a molar ratio of Ru: ir: ti is (20-35): (3-8): (60-75).
5. A titanium anode for electroplating according to claim 1 or 2, wherein the thickness of the intermediate layer is 2-15 μm.
6. A method for producing a titanium anode for plating according to any one of claims 1 to 5, characterized by comprising the steps of:
(1) dissolving acids or salts of Ru, Ir and Ti to prepare an intermediate layer coating solution; coating the intermediate layer coating liquid on a titanium substrate, drying and sintering to obtain an intermediate layer;
(2) dissolving at least one of Ta, Nb, Sn, Zr, Ti or Sb salt to prepare surface layer coating liquid; and (2) coating the surface layer coating liquid on the intermediate layer prepared in the step (1), drying and sintering to prepare a surface layer, thus obtaining the titanium anode for electroplating.
7. The method according to claim 6, wherein the dissolving process in the steps (1) and (2) is an alcohol dissolving process.
8. The method as claimed in claim 6, wherein the temperature of the drying step in the steps (1) and (2) is 100-150 ℃.
9. The method as claimed in claim 6, wherein the sintering temperature in step (1) and step (2) is 400-600 ℃.
10. Use of a titanium anode for electroplating according to any of claims 1 to 5 in electroplating.
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